Producing calcium hypochlorite compounds



Patented May 4, l926.

UNITED STATES PATENT OFFICE.

eu's'rav rrs'ron AND nnnmrcn nm'sz.

HEBMANN S. SCHULTZE, OF GRIESHEIM-ON-THE-MAIN, .AIID OF BITTEBFELD, GERMANY, ASSIGNORS TO THE GHEMISCHE FABBIK GBIESHEIH-ELEKTRQN, OI FRANKEOBT-ON-THE-MAIN, GERMANY.

PRODUCING CALCIUM HYPQCHLORI'IE COMPOUNDS.

.lto Drawing.

To all whom it may concern: Be it known that we, GUSTAV Prs'ron and HERMANN S. SGHULTZE, both citizens of Germany, and residing at' Griesheim-on-the- Main, Germany, and HEINRICH Rnrrz, a citlzen of Germany, and residing at Bitterfield, Germany, have invented certain new and useful Improvements in-Producing Calcium I-Iypochlorite Compounds, of which the following is a specification. V

This invention relates to the production of basic calcium hypochlorite compounds from chlorine, slaked lime and water. In our pending application Sr. No. 494,860 a process for producing basic hypochlorite com ounds is described according to. pro nets of difierent basicity areobtained by chlorinating lime in water, separating the so 'd bodies from the mother-liquor and drying them. Such products are of extraordinary value owing to their great stability. In this'process the proportions of the lime and chlorine employed or the composition of the precipitated basic hypochlorite com- 85 pounds must be continuously controlled in i order to determine the moment where the further introduction of chlorine is to be stopped in view of obtaining a determined roduct. We have found that by conductmg the chlorinating process in a determined direction based ona characteristic behaviour of the plercentage of the active chlorine in the mot er-liquor we are able to produce on a large scale and with satisfactory yield said basic hypochlorite compounds of well'defined character ora mixture of such compounds with neutral hypochlorite, such products beingidistinguished by excellent properties compared with the products of the type of ordinary bleaching powder.

In carrying out our improved process we may proceed for instance as follows Slaked lime and water are treated with chlorine in the usual way, the temperaturebeing allowed to rise to a moderate extent. After some time a solid body of basic character begins to precipitate which contains the active chlorine that was introduced, so that the proportion of active chlorine contained in the mother liquor diminishes. The introduction of chlorine is now continued until the proportion of active chlorine in the mother liquor begins to increase again. is reversing or minimum point is coinciding which Application filed Hoveinber 4, 1922. Serial 1%. 599,152.

with the moment when crystals exclusively of dibasis hyp'ochlorite'are found to form the precipitated body. Hereupon the introduction of chlorine is stopped The solid product is easily separated from the mother liquor by sucking, .centrifugating or pressing, and the separated 'mass is then dried. It is remarkable that the drying can be effected at elevated temperatures,

stance at 100 C. and more without any losses of chlorine being involved.

According to the above directions a prod.- uct is obtained the composition of which corresponds to the formula v,

20a (OI-I) 2'Ca(OCl) 2.

The microscopic test shows the precipitate as being constituted of well-formed hexagonal crystals whereby the product is confirmed to be a uniform chemical compound.

When the mass containing the dibasic body (which maybe of paste-like consistency) is further treated with chlorine, the proportion of active chlorine in the liquor will increase to a certain point, upon it will again decrease.- Now w chlorinating process is continued until the proportion of active chlorine in the mother liquor again increases,

wherea precipltate is obtained consisting almost uniformly of monobasic calcium hypochlorite This precipitate is obtained in the form of needle-shaped crystals and the microscopic test proves likewise its uniformity. The further treatment of the monobasic salt carried out corresponding to that of the dibasic one.- Finally, on treating the monobasic salt with chlorine in'its mother-liquor, the percentage of active chlorine in the said mother-liquor will increase again to a certain point and then decrease, pochlorite being formed in a solution of calcium chloride.

According to the present invention it will be possible to produce dibasic and menobasic calcium hypochlorites in a simple manner far superior to the known or common process of manufacturingbleachingpowder. For instance, our process may be carried out by means of completely closed apparatus which are far more compendious than the usual plant for making bleachingmother hen the.

such for inneutral hycerned.

powder, such apparatus presenting the further advantage that the workers are not incommoded by chlorine gas and dust. The products obtained by our process are by far superior to common-bleaching-powder, in so far as their contents of active chlorineand, more especially, their stability are conurth'ermore, they are of greater stability and better manageable than neutral calcium hy-pochlorite; they are even of excellent stability against elevated temper atures and moist air. The process disclosed by the present invention accomplishesa considerable advance in the manufacture of bleaching substances; inasmuch as uniformproducts are obtained in a'simple manner of manufacturing and with satisfactory yield, such products always containing the same proportion of actlve chlorine and being distinguished by hi h and constant stability and always equal y well adapted to be filtered ofi'.

en we do not intend to wait for the moment where the percentage of active chlorine in the mother-liquor attains its minimum point,- of course mixed products are obtained containing more or less, roportions ofthe former product and the al product according as the minimum point will be more or less attained. In this man-' ner, determined mixtures of the two products or of monobasic with neutral hypochlorites areobtained, that is to say mixtures containing any desired proportion of active chlorine.

The formation of uniform basic salts is bound to a determined concentration of active chlorine in the this determined concentration is somewhat variable in itself inasmuch as it depends on the concentration of the calcium chloride .slaked lime and water mother liquor, but

contained in the mother liquor, that is to say on the concentration of the mixture of For instance when starting from a mixture of 30 parts by weight of lime with 70 parts by weight of water the active chlorine in the mother liquor will amount to 42 grams per liter at the 'first minimum point, whilst such amount will be 55 grams when starting from a mixture of 27 parts of lime.

and 73 parts of water.-

at we claim as our invention and .de-

sirerto secure by Letters Patent is z- 1. Proess forregulating the percentage 0f active chlorine in the production of basic calcium hypochlorite compounds from chlorine, slaked lime and water which process consists in conducting the chlorination of the slaked lime according to the percentage of active chlorine in the mother-liquor in such a manner that the chlorination is stopped at the moments when the percentage of active chlorine in the mother-liquor has attained a minimum whereby a precipitate of a uniform substance is formed.

2. The process of manufacturing dibasic calcium hypochlorite, consisting in treating a mixture of slaked lime and water with chlorine until basic salt is precipitated, continuing the introduction of chlorine as long as the percentage of active chlorine in the mother-liquor is decreasing, stopping the chlorination when said percentage begins to increase and thereupon removing the mother-liquor and drying the remaining crystals. c

In testimony whereof we aflix our signaures.

HEINRICH REITZ.

originally employed. 

